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An ultrasound-assisted methodology for the determination of dissolved silicate in water has been developed by combining the miniaturized ion-associated based preconcentration method with energy dispersive X-ray fluorescence spectrometry (EDXRF). The method has been devised for the determination of silicate through molybdenum in the ion-associated complex between 12-molybdosilicate and crystal violet. Because silicate is determined indirectly via molybdenum fluorescent radiation the difficulties resulting from low fluorescence yield and low energy of silicon radiation were successfully overcome. A good ratio of silicon to molybdenum (1 to 41) and a sensitive Kα line of molybdenum make possible the determination of low concentration of silicon in the form of dissolved silicate. Under optimized conditions, good linearity, up to 5 μg of silicon in the form of silicate (r = 0.9990) and a detection limit of 9 ng mL−1 were achieved. The total RSD for the EDXRF determination of silicate, followed by precipitation of the ion-associated complex and its dissolution in a microdrop of isoamyl alcohol, was 6.5%. The enrichment factor was equal to 142. The developed method was used to determine the dissolved silica content in surface waters. The accuracy and repeatability of the proposed procedure were checked by the standard addition method and compared to the results obtained using the ICP-OES technique. The recovery (in the 93–97% range) was satisfactory and indicated the usefulness of the developed procedure. [ABSTRACT FROM AUTHOR]

The rapid development in nanomaterials and nanotechnologies has provided many new opportunities in the area related to analytical chemistry. In this paper the unique properties of these materials were used in order to preconcentrate heavy metals prior to detection by spectroscopic techniques. A novel, simple and highly reliable method for the preconcentration of trace amounts of chromium, manganese, cobalt, nickel, copper and zinc using electrochemically assisted sorption on oxidized multiwalled carbon nanotubes (MWCNTs) is developed. The proposed method is based on the application of an electric field to support the sorption process on oxidized MWCNTs. The proposed method was used to preconcentrate trace elements from water of pH = 4. After the preconcentration process, oxidized MWCNTs were directly measured using an energy dispersive X-ray fluorescence (EDXRF) spectrometer that reduces the number of chemicals required and minimizes sample handling. Besides EDXRF, any spectroscopy technique allowing the measurement of solid samples can be applied. The various parameters including pH of the solution, amounts of oxidized MWCNTs, sample volume and the influence of voltage as well as the time of assisted electric field on the sorption process were investigated for the optimization of the analytical procedure. Under optimized conditions the proposed preconcentration method offers a high recovery of 99% (Cr), 97% (Mn), 94% (Co), 96% (Ni), 92% (Cu) and 93% (Zn) and good precision of sample preparation (RSD) within 3.5–7%. If measurements are performed using the EDXRF spectrometer, the detection limits are 1 ng mL−1, 5 ng mL−1, 5 ng mL−1, 7 ng mL−1, 1 ng mL−1, 8 ng mL−1 for Cr(iii), Mn(ii), Co(ii), Ni(ii), Cu(ii) and Zn(ii), respectively. [ABSTRACT FROM AUTHOR]